CN117089295A - Heat dissipation buffer film and preparation method thereof - Google Patents
Heat dissipation buffer film and preparation method thereof Download PDFInfo
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- CN117089295A CN117089295A CN202311245748.3A CN202311245748A CN117089295A CN 117089295 A CN117089295 A CN 117089295A CN 202311245748 A CN202311245748 A CN 202311245748A CN 117089295 A CN117089295 A CN 117089295A
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- 230000017525 heat dissipation Effects 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 68
- 239000006260 foam Substances 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 16
- 238000012986 modification Methods 0.000 claims abstract description 16
- 239000004020 conductor Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 55
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- -1 alkyl triethoxysilane Chemical compound 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004472 Lysine Substances 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 239000004088 foaming agent Substances 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 claims description 3
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 claims description 3
- DMTRWFMFBIMXBX-UHFFFAOYSA-L lead(2+);6-methylheptanoate Chemical compound [Pb+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O DMTRWFMFBIMXBX-UHFFFAOYSA-L 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 4
- 230000003139 buffering effect Effects 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000002313 adhesive film Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 25
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940114081 cinnamate Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WBYWAXJHAXSJNI-VOTSOKGWSA-M trans-cinnamate Chemical compound [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a heat dissipation buffer film and a preparation method thereof, comprising the following steps: s1, preparing buffer foam slurry; s2, preparing a heat conducting material; s3, conducting heat conduction modification treatment of foam pulp; s4, depositing modified foam slurry; the method provided by the invention takes metal as a base, adopts a fixed formula, directly coats buffer foam on the surface, integrates the product structure, has the thickness of 80U-300U and the heat conductivity coefficient>50W/mK. is excellent in buffering and wave absorbing capacity and strong in adhesive property. For example, a product with a total thickness of 160U has a normal temperature peeling force of more than 2200gf/inch, a high temperature peeling force of more than 1100gf/inch, and a cohesive retention force of 85 DEG/1000 g at high temperature>24H, the ball falling absorption rate is more than 50%, and the volume resistance is low and can reach 10 9‑11 The light-shielding performance is good, and the transmittance of the adhesive film is lower than 0.3% at 550 nm.
Description
Technical Field
The invention relates to the technical field of functional metal film materials, in particular to a heat dissipation buffer film and a preparation method thereof.
Background
Along with the coming of the 5G age and the continuous upgrading of mobile phone functions, the trend of thinning and integrating internal parts of the mobile phone is obvious, the internal space is strictly limited, the performance and heat dissipation requirements of core parts are obviously improved, and a heat dissipation scheme suitable for the smart phone is developed towards the ultra-thin and efficient directions. As the bright spot technology of the 5G smart phone, the application of the OLED display screen is focused, unlike the conventional LCD display mode, the OLED display screen does not need a backlight source, and a very thin organic material coating and a glass back plate are adopted, so that when current passes through, the organic materials emit light, and the OLED display screen can be lighter and thinner, has larger visual angle, and has much smaller screen heating value than the conventional LCD screen when working for a long time. The heat dissipation scheme of the current 5G mobile phone is that a part of heat of the 5G mobile phone chip and other parts with serious heat generation is dispersed on an OLED screen in a heat radiation, heat conduction and even heat mode.
At present, the conventional buffer heat dissipation film on the OLED screen has the following problems: the thickness reduction space is small, and as two layers of adhesive structures are used for bonding different materials in the structure, the thickness of the adhesive is at least more than 2 mu m; the brittleness of the graphite flake is large, the external adhesive is required to be coated to prevent the graphite flake from being broken, the minimum thickness of the traditional artificial graphite flake is about 10 mu m, the thickness of the material is difficult to be further reduced by adjusting the thickness of the graphite flake, and the requirement of further ultrathin mobile phones cannot be met; the existence of the adhesive layer causes great interface thermal resistance between materials, which prevents heat transfer between interfaces; the coefficient of heat conductivity of the artificial graphite flake can reach 500w/m, and the coefficient of heat conductivity is seriously reduced because the graphite flake is entirely coated by the adhesive, so that the effect of uniform heat conduction is difficult to play, and the heat dissipation effect of the traditional heat dissipation buffer film is also poor.
Therefore, providing a heat dissipation buffer film and a method for preparing the same to solve the above-mentioned drawbacks is a major problem to be solved at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the heat dissipation buffer film and the preparation method thereof, and the heat dissipation buffer film prepared by the technical scheme provided by the invention has the advantages of excellent buffer absorption capacity and high bonding performance, and the thickness of the heat dissipation buffer film is 80U-300U, and the heat conductivity coefficient is more than 50W/mK.. Taking a product with the total thickness of 160U as an example, the normal temperature peeling force can reach more than 2200gf/inch, the high temperature peeling force can reach more than 1100gf/inch, the cohesive retention force can meet the high temperature of 85 ℃ per 1000g >24H, the falling ball absorptivity is more than 50%, the volume resistance is low, can reach 109-11, the light shielding performance is good, and the transmittance is lower than 0.3% under the condition of 550nm of a glue film.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the preparation method of the heat dissipation buffer film comprises the following steps:
s1, preparing buffer foam slurry:
s101, primary slurry preparation: taking 90-100 parts of acrylic resin according to parts by mass, stirring at 60-70 ℃, sequentially adding 25-40 parts of water, 1-5 parts of cross-linking agent, 2-4 parts of sodium dodecyl sulfate, a mixture of fatty alcohol polyoxyethylene ether sodium sulfate with a mass ratio of 2:1, 2-4 parts of KH792 silane coupling agent and 0.5-2 parts of catalyst, heating to 120-130 ℃, and stirring for 1-2 hours to obtain primary slurry;
s102, preparing foam raw pulp: cooling the obtained primary slurry to 50-60 ℃, sequentially adding 4-6 parts of foam stabilizer and 5-8 parts of foaming agent into the primary slurry, stirring for 2-3h, and cooling to normal temperature to obtain buffer foam slurry;
s2, preparing a heat conduction material: mixing 10-20 parts of modified graphene, 6-8 parts of silicon nitride and 5-10 parts of copper powder according to parts by mass, adding 70-80 parts of water for stirring treatment, sequentially adding 3-5 parts of alkyl triethoxysilane and 2-6 parts of gamma glycidyl ether oxypropyl trimethoxysilane in the stirring process, heating to 100-110 ℃, stirring for 1-1.5 hours, drying, grinding and sieving with 300-350 meshes to obtain a heat conducting material;
s3, conducting heat conduction modification treatment on foam slurry: continuously introducing rare gas with the purity of 99.99% into the buffer foam slurry prepared in the step S102, stirring the foam slurry at the same time, adding the heat-conducting material prepared in the step S2 into the foam slurry in the stirring process, stirring for 1-2h, stopping stirring and ending ventilation to obtain the foam slurry after the heat-conducting modification treatment;
s4, depositing modified foam slurry: and (3) depositing the foam slurry prepared in the step (S3) on the surface of the substrate after the heat conduction modification treatment, wherein the deposition thickness is as follows: 80U-300U, heating to 150-160 ℃, maintaining for 0.5-1h, and cooling to normal temperature to obtain the heat dissipation buffer film.
Preferably, in S101, the cross-linking agent is selected from one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, polyethylene, polyvinyl chloride, chlorinated polyethylene, and polystyrene.
Preferably, in S101, the catalyst is one of 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane platinum, dibutyltin dilaurate, and lead isooctanoate.
Preferably, in S102, the foam stabilizer is one or more selected from dodecyl dimethyl amine oxide and alkyl alcohol amide.
Preferably, in S102, the foaming agent is one or more selected from calcium carbonate, silicon carbide and carbon black.
Preferably, in S2, the preparation process of the modified graphene is as follows: mixing 10-20 parts of graphene with 3-5 parts of lysine according to mass parts, stirring for 1-2 hours, then placing into 80-100 parts of concentrated sulfuric acid with the concentration of 2-10moL/L, placing into a polytetrafluoroethylene autoclave, performing hydrothermal reaction for 7-9 hours at 170-220 ℃, filtering, washing and drying to obtain the modified graphene oxide.
Preferably, in S3, the rare gas introduced is argon, and the gas flow rate is: 11-17L/min.
A heat dissipation buffer film comprises a substrate layer and a modified foam layer.
Compared with the prior art, the invention has the beneficial effects that:
1. the heat dissipation buffer film prepared by the technical scheme provided by the invention has the thickness of 80U-300U and the heat conductivity coefficient>50W/mK. is excellent in buffering and wave absorbing capacity and strong in adhesive property. Taking a product with the total thickness of 160U as an example, the normal temperature peeling force can reach more than 2200gf/inch, the high temperature peeling force can reach more than 1100gf/inch, and the cohesive retention force can meet the high temperature of 85 ℃/1000g>24H, the ball falling absorption rate is more than 50%, and the volume resistance is low and can reach 10 9-11 The light-shielding performance is good, and the transmittance of the adhesive film is lower than 0.3% at 550 nm.
Drawings
FIG. 1 is a flow chart of a process for preparing a heat dissipation buffer film of the present invention;
fig. 2 is a flow chart of a process for preparing the buffered foam slurry of the present invention.
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which it is shown, however, to illustrate some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-2, the present invention provides a technical solution:
example 1
S1, preparing buffer foam slurry:
s101, primary slurry preparation: taking 90 parts of acrylic resin by mass and stirring at 60 ℃, sequentially adding 25 parts of water, 1 part of propyl orthosilicate, 2 parts of sodium dodecyl sulfate, a mixture of sodium fatty alcohol polyoxyethylene ether sulfate with the mass ratio of 2:1, 2 parts of KH792 silane coupling agent and 0.5 part of dibutyltin dilaurate, heating to 120 ℃, and stirring for 1h to obtain primary slurry;
s102, preparing foam raw pulp: cooling the obtained primary slurry to 50 ℃, sequentially adding 4 parts of dodecyl dimethyl amine oxide and 5 parts of silicon carbide into the primary slurry, stirring for 2 hours, and then cooling to normal temperature to obtain buffer foam slurry;
s2, preparing a heat conduction material:
s201, preparing modified graphene: mixing 10 parts of graphene and 3 parts of lysine according to mass parts, stirring for 1h, then placing into 80 parts of concentrated sulfuric acid with the concentration of 3moL/L, placing into a polytetrafluoroethylene autoclave, performing hydrothermal reaction for 7 hours at 220 ℃, filtering, washing and drying to obtain modified graphene oxide;
s202, assembling a heat conduction material: mixing 10 parts of modified graphene, 6 parts of silicon nitride and 5 parts of copper powder according to parts by mass, adding 70 parts of water for stirring treatment, sequentially adding 3 parts of alkyl triethoxysilane and 2 parts of gamma glycidyl ether oxypropyl trimethoxysilane in the stirring process, heating to 100 ℃, stirring for 1h, drying, grinding and sieving by 300 meshes to obtain a heat conduction material;
s3, conducting heat conduction modification treatment on foam slurry: continuously introducing argon with the purity of 99.99% into the buffer foam slurry prepared in the step S102, wherein the gas flow is 11L/min, stirring the foam slurry, adding the heat-conducting material prepared in the step S2 into the foam slurry in the stirring process, stirring for 1h, stopping stirring, and ending ventilation to obtain the foam slurry after the heat-conducting modification treatment;
s4, depositing modified foam slurry: and (3) depositing the foam slurry prepared in the step (S3) on the surface of the substrate after the heat conduction modification treatment, wherein the deposition thickness is as follows: 160U, heating to 150 ℃, maintaining for 0.5h, and cooling to normal temperature to obtain the heat dissipation buffer film.
Example 2
S1, preparing buffer foam slurry:
s101, primary slurry preparation: taking 100 parts of acrylic resin according to mass parts, stirring at 70 ℃, sequentially adding 40 parts of water, 5 parts of chlorinated polyethylene, 2 parts of sodium dodecyl sulfate, a mixture of sodium fatty alcohol polyoxyethylene ether sulfate with a mass ratio of 2:1, 2 parts of KH792 silane coupling agent and 2 parts of lead isooctanoate, heating to 130 ℃, and stirring for 2 hours to obtain primary slurry;
s102, preparing foam raw pulp: cooling the obtained primary slurry to 60 ℃, sequentially adding 6 parts of alkyl alcohol amide and 8 parts of calcium carbonate into the primary slurry, stirring for 3 hours, and cooling to normal temperature to obtain buffer foam slurry;
s2, preparing a heat conduction material:
s201, preparing modified graphene: mixing 20 parts of graphene and 5 parts of lysine according to mass parts, stirring for 2 hours, then placing into 100 parts of concentrated sulfuric acid with the concentration of 10moL/L, placing into a polytetrafluoroethylene autoclave, performing hydrothermal reaction for 9 hours at 220 ℃, filtering, washing and drying to obtain modified graphene oxide;
s202, assembling a heat conduction material: mixing 20 parts of modified graphene, 8 parts of silicon nitride and 10 parts of copper powder according to parts by mass, adding 80 parts of water for stirring treatment, sequentially adding 5 parts of alkyl triethoxysilane and 6 parts of gamma glycidyl ether oxypropyl trimethoxysilane in the stirring process, heating to 110 ℃, stirring for 1.5 hours, drying, grinding and sieving by 300 meshes to obtain a heat conduction material;
s3, conducting heat conduction modification treatment on foam slurry: continuously introducing argon with the purity of 99.99 percent into the buffer foam slurry prepared in the step S102, wherein the gas flow is 17L/min, stirring the foam slurry at the same time, adding the heat-conducting material prepared in the step S2 into the foam slurry in the stirring process, stirring for 2 hours, stopping stirring, and ending ventilation to obtain the foam slurry after the heat-conducting modification treatment;
s4, depositing modified foam slurry: and (3) depositing the foam slurry prepared in the step (S3) on the surface of the substrate after the heat conduction modification treatment, wherein the deposition thickness is as follows: 300U, heating to 160 ℃, maintaining for 1h, and cooling to normal temperature to obtain the heat dissipation buffer film.
Example 3
S1, preparing buffer foam slurry:
s101, primary slurry preparation: taking 95 parts by mass of acrylic resin, stirring at 65 ℃, sequentially adding 30 parts by mass of water, 3 parts by mass of polystyrene, 3 parts by mass of sodium dodecyl sulfate, a mixture of sodium fatty alcohol polyoxyethylene ether sulfate with a mass ratio of 2:1, 1 part by mass of KH792 silane coupling agent, 1 part by mass of 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane platinum, heating to 125 ℃, and stirring for 2 hours to obtain primary slurry;
s102, preparing foam raw pulp: cooling the obtained primary slurry to 55 ℃, sequentially adding 5 parts of alkyl alcohol amide and 7 parts of carbon black into the primary slurry, stirring for 2.5 hours, and cooling to normal temperature to obtain buffer foam slurry;
s2, preparing a heat conduction material:
s201, preparing modified graphene: mixing 15 parts of graphene with 4 parts of lysine according to mass parts, stirring for 1.5 hours, then placing into 90 parts of concentrated sulfuric acid with the concentration of 8moL/L, placing into a polytetrafluoroethylene autoclave, performing hydrothermal reaction for 8 hours at 200 ℃, filtering, washing and drying to obtain modified graphene oxide;
s202, assembling a heat conduction material: mixing 15 parts of modified graphene, 7 parts of silicon nitride and 8 parts of copper powder according to parts by mass, adding 75 parts of water for stirring treatment, sequentially adding 4 parts of alkyl triethoxysilane and 4 parts of gamma glycidyl ether oxypropyl trimethoxysilane in the stirring process, heating to 105 ℃, stirring for 1.5 hours, drying, grinding and sieving by 300 meshes to obtain a heat conduction material;
s3, conducting heat conduction modification treatment on foam slurry: continuously introducing argon with the purity of 99.99% into the buffer foam slurry prepared in the step S102, wherein the gas flow is 14L/min, stirring the foam slurry at the same time, adding the heat-conducting material prepared in the step S2 into the foam slurry in the stirring process, stirring for 2 hours, stopping stirring, and ending ventilation to obtain the foam slurry after the heat-conducting modification treatment;
s4, depositing modified foam slurry: and (3) depositing the foam slurry prepared in the step (S3) on the surface of the substrate after the heat conduction modification treatment, wherein the deposition thickness is as follows: 160U, heating to 155 ℃, maintaining for 1h, and cooling to normal temperature to obtain the heat dissipation buffer film.
Comparative example
Comparative example 1:
comparative example 1 differs from example 1 only in that the step S101 originally present in example 1 was partially omitted in comparative example 1, and thus the step of adding "propyl orthosilicate, dibutyltin cinnamate" was omitted, and the remaining steps were identical in comparative example 1 and example 1.
Comparative example 2:
comparative example 2 is different from example 1 only in that the step S101 originally present in example 1 was partially omitted in comparative example 2, so that the step of adding "a mixture of sodium dodecyl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate in a mass ratio of 2:1" was omitted, and the remaining steps were identical in comparative example 2 and example 1.
Comparative example 3:
comparative example 3 is different from example 1 only in that the step S201 originally existing in example 1 is partially omitted in comparative example 3, so that the step of "preparation of modified graphene" is eliminated, and the remaining steps are exactly the same as in comparative example 3 and example 1.
Comparative example 4:
comparative example 4 is different from comparative example 2 in that only the step S201 originally present in comparative example 2 was partially omitted in comparative example 4, thereby eliminating the step of "preparation of modified graphene", and the remaining steps are identical in comparative example 4 and comparative example 2.
The peel force at normal temperature and the peel force, cohesion and heat conductivity at high temperature (85 ℃) of examples 1 to 3 and comparative examples 1 to 4 were measured; the transmittance of examples 1 to 3 and comparative examples 1 to 4 was measured at 550nm, and the measurement results are shown in the following table:
the surface of the detection result in the table shows that the parameters such as the peeling force at normal temperature/high temperature, the cohesive force at high temperature, the heat conductivity coefficient, the falling ball absorptivity and the passing rate under 550nm of the embodiment 1-3 are all obviously superior to those of the comparative embodiment 1-4, so that the heat dissipation buffer film material prepared by the technical scheme provided by the invention is reliable, and meanwhile, the parameters such as the peeling force at normal temperature/high temperature, the cohesive force at high temperature, the heat conductivity coefficient, the falling ball absorptivity and the passing rate under 550nm of the embodiment 1-3 are all obviously superior to those of the comparative embodiment 1-4, and particularly, the great difference between the parameters of the embodiment 1 and the comparative embodiment 4 can prove that the peeling force, the cohesive force, the heat conductivity coefficient and the buffering performance of the metal film material can be obviously improved on the basis of using the brand-new coating material, the normal temperature peeling force can reach more than 2200gf/inch, the high temperature peeling force can reach more than 1100gf/inch, the cohesive force can meet the requirements of high temperature/1000 g, the heat absorption rate is more than 50nm, the heat dissipation buffer film material has the heat conductivity is more than about 109.109 nm, and the heat absorption efficiency is more than the prior art has wide, and the heat absorption efficiency is better than the heat absorption of the heat absorption is more than about 11 nm, and has the heat absorption efficiency is better than the heat absorption is more than the heat absorption of the heat absorption is more than has.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the heat dissipation buffer film is characterized by comprising the following steps of:
s1, preparing buffer foam slurry:
s101, primary slurry preparation: taking 90-100 parts of acrylic resin according to parts by mass, stirring at 60-70 ℃, sequentially adding 25-40 parts of water, 1-5 parts of cross-linking agent, 2-4 parts of sodium dodecyl sulfate, a mixture of fatty alcohol polyoxyethylene ether sodium sulfate with a mass ratio of 2:1, 2-4 parts of KH792 silane coupling agent and 0.5-2 parts of catalyst, heating to 120-130 ℃, and stirring for 1-2 hours to obtain primary slurry;
s102, preparing foam raw pulp: cooling the obtained primary slurry to 50-60 ℃, sequentially adding 4-6 parts of foam stabilizer and 5-8 parts of foaming agent into the primary slurry, stirring for 2-3h, and cooling to normal temperature to obtain buffer foam slurry;
s2, preparing a heat conduction material: mixing 10-20 parts of modified graphene, 6-8 parts of silicon nitride and 5-10 parts of copper powder according to parts by mass, adding 70-80 parts of water for stirring treatment, sequentially adding 3-5 parts of alkyl triethoxysilane and 2-6 parts of gamma-glycidyl ether oxypropyl trimethoxysilane in the stirring process, heating to 100-110 ℃, stirring for 1-1.5 hours, drying, grinding and sieving with 300-350 meshes to obtain the heat conducting material;
s3, conducting heat conduction modification treatment on foam slurry: continuously introducing rare gas with the purity of 99.99% into the buffer foam slurry prepared in the step S102, stirring the foam slurry at the same time, adding the heat-conducting material prepared in the step S2 into the foam slurry in the stirring process, stirring for 1-2h, stopping stirring and ending ventilation to obtain the foam slurry after the heat-conducting modification treatment;
s4, depositing modified foam slurry: and (3) depositing the foam slurry prepared in the step (S3) on the surface of the substrate, wherein the deposition thickness is as follows: 80U-300U, heating to 150-160 ℃, maintaining for 0.5-1h, and cooling to normal temperature to obtain the heat dissipation buffer film.
2. The method for preparing a heat dissipation buffer film according to claim 1, wherein in S101, the cross-linking agent is one or more selected from the group consisting of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, polyethylene, polyvinyl chloride, chlorinated polyethylene, and polystyrene.
3. The method for preparing a heat dissipation buffer film according to claim 1, wherein in S101, the catalyst is one of 1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane platinum, dibutyltin dilaurate, and lead isooctanoate.
4. The method for preparing a heat dissipation buffer film according to claim 1, wherein in S102, the foam stabilizer is one or more selected from dodecyl dimethyl amine oxide and alkyl alcohol amide.
5. The method for preparing a heat dissipation buffer film according to claim 1, wherein in S102, the foaming agent is one or more selected from the group consisting of calcium carbonate, silicon carbide, and carbon black.
6. The method for preparing the heat dissipation buffer film according to claim 1, wherein in S2, the preparation process of the modified graphene is as follows: mixing 10-20 parts of graphene with 3-5 parts of lysine according to mass parts, stirring for 1-2 hours, then placing into 80-100 parts of concentrated sulfuric acid with the concentration of 2-10moL/L, placing into a polytetrafluoroethylene autoclave, performing hydrothermal reaction for 7-9 hours at 170-220 ℃, filtering, washing and drying to obtain the modified graphene oxide.
7. The method for preparing a heat dissipation buffer film according to claim 1, wherein in S3, the introduced rare gas is argon, and the gas flow is: 11-17L/min.
8. A heat dissipation buffer film, characterized in that the heat dissipation buffer film is made by the preparation method of any one of claims 1-7, and the heat dissipation buffer film comprises a substrate layer and a modified foam layer.
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| CN114774032A (en) * | 2022-05-11 | 2022-07-22 | 广东思泉新材料股份有限公司 | Buffer and shock-absorbing heat dissipation foam and preparation method thereof |
| CN116218444A (en) * | 2023-02-16 | 2023-06-06 | 诸暨市科凌新材料科技有限公司 | Modified silane sealant containing graphene |
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| JPWO2016152660A1 (en) * | 2015-03-23 | 2018-01-11 | 積水化学工業株式会社 | Acrylic resin heat dissipation foam sheet |
| KR102203001B1 (en) * | 2018-12-21 | 2021-01-14 | 한국과학기술원 | Porous Structure-based Graphene Foam and Method of Preparing the Same |
| CN115678091B (en) * | 2022-02-08 | 2024-02-27 | 广东思泉新材料股份有限公司 | Acrylic foam and preparation method thereof |
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| CN114774032A (en) * | 2022-05-11 | 2022-07-22 | 广东思泉新材料股份有限公司 | Buffer and shock-absorbing heat dissipation foam and preparation method thereof |
| CN116218444A (en) * | 2023-02-16 | 2023-06-06 | 诸暨市科凌新材料科技有限公司 | Modified silane sealant containing graphene |
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